반응 #514365

ord-2ddbeaa9cf7b4e8da7dd44bf9c41cde8

반응 방정식

NC(N)=C([N+](=O)[O-])[N+](=O)[O-]
1,1-diamino-2,2-dinitroethylene
O=[N+]([O-])O
nitric acid
CC1=NC(=O)C(=O)C=N1
2-methyl-4,5pyrimidindione
O
water
CC1=NC(=O)CC(=O)N1
2-methyl-4,6-pyrimidindione
수율 35.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITWithin a few seconds
  2. 2
    세척The precipitate were washed with water
  3. 3
    기타dried at 50° C
  4. 4
    기타2.6 g 1,1-diamino-2,2-dinitroethylene was recovered (35% yield)

실험 절차

Finely ground 2-methyl-4,5pyrimidindione (5.1 g, 0.05 mole) was dissolved in concentrated sulphuric acid (40 ml, 1.84 g/cm3) at 15-20° C. during vigorous stirring. At the same temperature nitric acid (8.0 ml, 1.52 g/cm3) was added over a 30-min period. After 3 h, the reaction mixture was poured into water. Within a few seconds, bright yellow crystals settled out (1,1-diamino-2,2-dinitroethylene). The precipitate were washed with water and dried at 50° C. 2.6 g 1,1-diamino-2,2-dinitroethylene was recovered (35% yield).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06312538B1uspto-grants-2001_11